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04’

Memorandum Report

Preliminary Operating Mam*el -Hanfracture of Adipic Acid

Introduction:

*•' * This manuel covers the operating details for the C**.^*-^
manfacture of pure adipic acid from .gexalln . The procedure
Is covered in five sections as follows: _

1. Vapor phase OXIDATION of Bexalin.

22. Refining of cyclo hexanone from vapor phase Ctxida-

-tion. V~ ~

3. Liquid phase Oxidation of Cyclohexanone to Adipic

44. Purification of AdipiA acld*-from liquid phase

0 xidation.

6 * Recovery of Acefltcacid and Adipic acid and from '
purge liquor.

* 2 <

n>

*

^Vjnary of Process Materials £)

Materials Per. Hay Quanities Perlr.

per month ;

Adipic acid 775 # — 21,000 # 250,000#

Acetic acid 145 # — 4,000 # 48 ,000 #

Cyclohexanone — - — 91 gals. - — 2,500 gals.-— — 50,000 gals.

Eexalin 116 gals. - — 5, 200 gals . 58,000

Manganese Acetate — 1.7# 47 # 560 #

Darco 17 # 470# 5,600 #

Acetic acid make -up will be required at this rate,
once the system is completftjy filled. Approximately 5,000 lbs.
of Acetic acid will be required when first starting the process*
At least four feed mixes will be made before any recovered
Acetic acid is available.

,>.C.

■£.

Part l. v Vapor Phase Oxidation of dexalin

— ... r

to Cyclohexanone*

Discussion of Safety Precautions* ^ ' .

. 1* Bexalin and Cyclohexanone are Inflammable materl—

•ala* Explosion proof motors and lamps are used. There should I- ,
not he smoking or open flames in this area. Also avoid bringing
these materials in contact with the akln^

Outline of Process*

Vapor phase oxidation is accomplished by passing
Hexalin vapor and air over silver gauze Catalyst, which operates
at about 550 C. Although the reaction is slightly exothermic
the converter is not self sustaining. External heat must be
applied. The off vapora are condensed and decanted into m '
water saturated Cyclohexanone layer and a Cyclohexanone saturated
water layer. The off gases are cooled and vented toaatmosphere
A flow diagram of the process is attached { Figure 1), -

Detailed Operating jlnatructlons *

(A) Starting the process

1* Since the freezing poi nt of Hexalin ie approx-
-imately 25 C. the hexalin storage and all lines through which
Hexalin passes mu at b« steam heated and lagged. The temperature
of Hexalin feed tank Mo. 5-A must be held between 50 and 55 C*
Turn steam on feed tank So. S-A and all steam traced lines.

,2. Fill Hexalin feed No. 5-A wltto tkf ihedru Hsiallnilnes
from the tank ftfrm* ' *

‘ 5. Turn water on converter NO. 4-A. .-IriVL-'.

4. Check decanter No.5 and see thatv valves are set
to put. oil layer to No. 7 storage and water layer to No. 6 storage
• 5. Turn full steam on vaporizer No. 5-B.

^-cont. from page 3

6. Start air compressor. \

7. Start Hexalin feed pump Bo. 3-D.

S. Turn heat on converter Bo. 3 -C and heat to 600 C. . rr‘ -i- -
9. Start flow of Hexalin of 3 to 4 G.F.H. to vaporiser, 'y -

<^lo . “Start very small flow of air to vaporiser .( Hot more ■

then 2 to 3 cu. ft. per. min.)

11 • As reaction flights Off 1 ' gradually increase air flow
to hold converter between 600 and 650 C.

12. Gradually raise Eexalin feed to 6 or 6 G.P. H.and
Increase air flow to correspond.

1 13. Check condenser No.4-A to be sure it is operating.

14. If at any time the Hexalin flow is stopped, turn off
all flow immediately.

Shutting Down the Process.

1. Stop air flow to converter.

2.8 tpp Hexalin flow to vaporiser.

3, Hexalin feed pump MO. 3- A.

.4. Turn heat off condenser. • , , •

6. Turn steam off vaporiser.

6. Turn cooling water off condenser. _ ~

Bo. 4-A (Caution^ In freezing weather leave
small flow of water on condenser, if shut down is to be -for
some time, condenser and water lines ahpuld be drained).

.* > . 1 A - / *

C. ■ Control *£T Process . ‘ */•

Mo control is required for the vapor phase
oxidation beyond maintenance of. uniform flows of air and
Hexalin being fed. Operating temperature of the convertor

/T cont. from page *.•' “

C V) "* I J//

must be between 500 and 550 C. It is necessary to supply s yj*
some external heat to the converter * -

As a general check on conversion and performance o
the unit the laboratory should analyze thee crude product - ^
by precession distillation* Occasional analyses should be
made of the off gas, to check the loss of material is CO
and COjf* . . . .

Part 12. Refining of Cyclohexanone
Outline of Process

The crude Cyclohexanone produced in the vapori^phasa
oxiddation is refined in a 200 gallon vacuum still. The process
consists of drying the charge by refluxing through adecanter,
producing a refined ketone fraction^ aAaeml -refined ketone
fraction, and a hexalin residue which Is returned to hexalin
storage.

Distillation Procedure:

See Pig. “2 for flow diagram.

A. Production of Refined Cyclohexanone from vapor^/
phase Oxidation.

1. Chargp still NO. 10 -A. to approximately one
Inch from top of sight glass with crude Cyclohexanone from
No. 7 tank.

2^ Turn water on ketone still condenser No *10 -O'.

5. Be sure that still is vented through valvel. l.“
at base of 10-B. -

’ v ' 4. Turn full steam on coils to NoilO -A Itetfcla

and beat to about 80 C. Reduce ateam flow to about 100 lbs.1^ :

per. hour and bring still to reflux. ' * ''-‘v

■ U J

5. Set valve so that make passed to decanter Nol 10-B
water layer to water storage aNo. 6 and oil layer returned to

still kettle

T , O ' •

6. Decant water continuously at app» miraately 2:1

M€

F

reflux ratio. The proper draw off is that which gives the

,/ •

maximum water removal. „ .

V-\.' 7. When head temperature reaches 100 C. and no more

water will separate turn off steam to kettle. - . d

8. Close valve to decanter Bo 10-D and prepare still
for vacuum operation.

9. Close valve on oil return to kettle.

10. Start vacuum pump as instruced below and gradu- •
-ally reduce pressure on system .{At such a rate the normal
boil up is maintained to 2.0 inches H. g.

11. The foil owing ivcut s are made:

A. 1. ."i Prom water cut to R.l - 1. 4520

at 15.6 C. at a 4:1 reflux ratio - to crude ketone storage
Bo. 7.

1£2 B. Prom S. I. equals 1.452 to 1.453 at 15.6 C.

at 2:1 reflux ratio to refined ketone storage Bo. 12

C. From R.l equals 1^530 to 1.4540 at 15660
at 4:1 reflux ratio to refined ketone storage Ho. 12.

D. From R.l. equals 1.4540 to a head temper-

-ature of 88 to ® 0 C. (at 21nch Hg.) at 4:1 reflux ratio to
crude ketone storage Bo.l. .

E. The still residue is pumped { Bo. 9 pump*)
to crude hexalin storage at the hydrogenation plant.

12. The actual distillation procedure made , vary aom-
-ewhat from the above depending upon the quality of the crude
cyclohexanone charge. For low grades of crude ketone it will "
be necessary to take a semi - refined ketone out to be fed in
a semi-. refined storage Mo. 11 for redistillation

r ' j " ■ '

C O tJt)

Figure 0 gives the boiling point pressure curves for cycl-

-ohexanone and hexalin.

Fig. 4 gives a pivot distillation of crude cyclohexanone ;:r
as produced by vapor phase oxidation. ■

Recovery of oil from Cyclohexanone water layer,

1. Charge still Wo. 10-A approximately li- inch below . .
the top of sight glass with water layer Bo* 6 tank*

2. Turn water on ketone still condenser Bo. 10 -C
53 . Turn steam on kettle and establish reflux.

4 . Pass draw off through decanter returning water
layer to still kettle and oil layer to crude ketone storage
Bo.7. The rate of draw off is set to give the maximum removal
Of oil.

5. When all oil has been removed shut down and discharge
water im kettle to sewer.

Vaouum Pump Operation.

1. See that the oil is at the proper level in the oil
separator tank. The proper oil is Opalube S.A.E 20 for winter
operation and Opalube 8.A.E.30 for summer operation.

2. To start Vacuum Pump.

A. Start small flow water to water Jacket.

B. Seevthfet all valves in oil seal line are closed

and remain closed untill pump is running. ; .

— - C. Turn on power and start pump running.

D. Open wide plug cock in oil seal line.

E. Open one and one - half turns the valves allowing
oil to flow into bearings, at each end of crank shaft.

P. Suction linea should be absolut^Mr free of all 1
foreign materials and should be perfectly tight.

w:

'M

Shutting down Pump.

A. Close plug, cock in oil seal line.

B. Allow pump to run thirty seconds to free itself of oil.

C. Shut off power. r- -~

D. Stop flow of cooling water to jacket.

Part S. Liquor Phase Oxidation of Cyclohexanone to Adipic Acid.

Outline of Process*

Adipic acid is made from cyclohexanone by
liquid phase oxidation. Air and cyclohexanone in an acetic acid
medium are upssBaddco-current through unpacked towers in aeries.

The towers are maintained at 80 C. by water circulation.

The adipic acid solution formed is collected In a
hold up tank for subsequent purification. The spent air is
first water cooled and then passed through a refrigerated
condenser to remove acetic acid and cyclohexanone. The conde-
nsate is returned to the oxidisera with the feed.

Ai flow diagram is attached • Pig. 6.

1* Acetic cacid Storages The 200 gallon aluminum tank So .15
Is provided for acetic acid storage. Since ita only source of ~
acetic acid la from the acid recovery still, thia tank will be
empty, when first starting the process. "^-dv '

2. Acid mother Liquor Storage* This storage So. 34 tank
will also he empty when first starting the prpcess. Its source
of acid liquor is from the centrifuge.

3. Refined Ketone Storage; The refined ketone storage Ko.12
should contain at least 50 gallons of refined ketone as produ-
ced in Section 2. above.

4. Content of Oxidizers: If oxidizers are empty add to No.20-A
oxidizer, about 65 gallons of pure acetic acid from carboya.

This Is done as follows:

A. Pump 75 gallons acetic acid from cartoje titta’ough

pump No. 18 -B to feed tank No.20-C. ■_ _ _

B. Pump acid from feed tank through pump No.20-B:to
oxidizers. If oxidizers are full from some previous shut-down
they can usually be started without any charge.

P§.; Preparation of the Fill l L

The feed Is mixed in weigh tank No. 18 and is suff-
■ Icient to last for twelve hours. The normal feed mix consists
Of the following:

A. Pure acetic acid from No. 13 tank equals 335#

B • Refined ketone from No. 12 tank 360# '

C. Acid mother liquor from No. 34 tank * 800#.

^ ‘ ' 1495#

{ Approx.l74gals )

Catalyst equals 81bs. manganese acetate dissolved

in Acetic acid, per batch.

{/ftp

Since It i/^ecessary to add approximaO-y 85 lbs pf nake- pt?
-up acetic acid every 12 hours, the catalyst is dissolved , In the
quanlty of acid In a carboy afad pumped to the weigh tank* The
remaining acetic acid required, (335)lbs. la run in from the,^.-.
acetic acid storage. . .yXTzX

When first starting the process there will be no acetic acid .
In Wo. 13 tank and no acid mother liquor in Ko.34 tank. The
composition of these mixes will be as follows:

Pure Acetic acid from carboys equal 1135#

Refined Cyclohexanone from Wo. 12 tank equals 360# * - .

Total 1495#

Catalyst equals 8# maganese acetate dissolved In 85 lbs.
of acetic acid, all of the acid and catalyst from the first
mixes la pumped directly from carboys to the weigh tank. Rubber -
gloves and goggles should be used during this operation.

6. when the feed mix has been completed, circulate mix th-
orough pump Wo.lS-B to top Of Wo. 16 tank for two hours.

P 7. PumpV.feed fcbrfeidt tagksJiefcfiG-e.

B • Water“Circulatlng system.

Pill water hold up tank Wo.20-2 with fllteredrwAber

and circulate water through oxidizers.

• 9. Turn water on cooler Bo.20-F*

10. Tuna ammonia on refrigerated3Col^mn W0.20-H. 1

11. 8 tart feed pump Ho.20-D. : -.,■■■ - ■,

12 .

Start air compressor and set flow at 27 cu. ft .per. min.

'

, to oxidizers. '

•• .

*13. Turn small steam flow on, feed preheater »o.20-». -

>7 ;

*>14. Start feed or about 6 G.P.H to oxidizers.

15* Adjust water circulating system to hold oxidizers at 80 C.
16. When feed has settled out at G.P.H. gradually raise to
14 G.P.H. i

17. Check of recycle condensate frcC) separator So.20-M

and 20»G. Leave rotameters wide open so that full flow returns
to oxidizers.

18. Be sure that steam Is on coll of hold up tank No.20-J. *nd
all steam traced lines In this system. These lines should always
he heated unless system is flushed and completely dra lned 'ir-TL w

19. Control of process consists of malntainlnge constant flows
of 'll quid feed and air and holding the oxidizer at 80 C*

Shutting down the Process.

1. Cut off feed to oxidizers.

2. Stop air flow to oxidizers, and shut down air comprea so r

if not needed for vapor phase oxidation or isobutyl propoxate

-it

5. Shut down feed pump No.20-D.

4. Cut steam off preheater No. 20-N.

5. Stop cooling water to cover No.20-L and start a small
steam flow to the water circulating system, or completely drained
to hold up tank No. 20-J. If the shut down la to he for some
time the oxidizers should be drained.

6. Turn water off spent air cooler No. 20-F. (Caution:

Leave small flow of water on this condenser in freezing weather*
or drain completely).

7. Turn ammonia off refrigerated apent air cooler.

YOU WILL FIND ANALYTICAL METHODS ON SEPARATE SHEETS.

’ C w Part
oxidation.

4. Purification of adipic acid from liquid phase

Outline of Process;

The effluent from the mother phase oxidizers
Is cooled In batch crystallizer and the adipic acid which crystal-
-11* es is centrifuged from the solvent medium and washed.; r

The crude ^ibed crystals are dissolve<Qji distilled water
and recycled mother liquor with a proportionate amount or
second crude crystals and treated with Darco. The hot liquor
is filtered free of Darco and slowly cooleddin a second batch
crystallizer. The adipic acid crystals obtained are ©entrifu-
-ged from the mother liquor washed, and dried. The Mother liquor
from this step is divided into two portions. One portion is
held in the water solution tank for dissolving additional adi-
pic acid. The other portion purged to a recovery evaporator*
where water and acetic acid are removed and adipic acid is
recovered from the residue ae second crude crystals.

A flow diagram ie attached Fig. 6.

P

Summary of Operating Instructions *

A. Separation of first grade crude crystals from
acid mother liquor.

1. Be sure that all lines from hold up tank Mo.“20-J
to crystallizer No. 30 are heated.

2. Fill water jacket of No. 30 Crystallizer and heat
to 80 C. with a team.

3. Check distilled water supply, at least BO gallons
should be on hand.

4. Pump acid solution from Mo.20-J to Jlo.30
crystallizer. Charge should be 250 to 300 gallons. '

5. Start slow speed stirrer in No.30

■ 6. Start flows of cooling water to No. SO jacket*

Adjust cooling water rate to give cooling of approximately
10 C per hour*

7* Then the acid liquor in No. 50 has crystallized
and colled to 20 C., Check centrifuge No. 51 to be sure it will
operate pro# 61 *!?*

13

Place eruae adipic acid crystal reclver under centrifuge

Wt’

ft*

discharge*

; . / • '••••- ^.4.

81 The centrifuging Is done on the following eyelet
l '2 < A. Set liquor valves to acid mother liquor storage B052.

B. Start centrifuge on alow speed and charge fronTHo.SO/y

crystallised* When cake begins to build up near the top of the
basket, atop flow from Wo. 50 .

C. Put centrifuge on high speed for one minute. ' v '^y/

P* Put centrifuge on alow spped. k'

B* Set liquor valves to water mother llqutr storage No. 54.

F. Wash crystals with three gallons of distilled water*

G. Put centrifugeo on high apeed for one minute.

H. Put oentrlfuge on low speed and discharge basket to
crude crystal recfctver.

Repeat the above cycle as many times as it is nec- -
essary to empty Ko*50 crystalliser. A 500 gallon charge to Ho*50
should be handeled In about eight loads to the centrifuge* .

9. When charge has been centrifuged, wash centrifuge wtth
five gallons of distilled water. Rtn wash water to No.54 tank.

B. Purification and Prying of first grade crude crystals.

1* Besure steam Is on heating element in water
solution tank No. 41 and all steam traced lines. ~

2. Check distilled water supply, at least 150 gallons
.should be on hand,

■ 5. To No.41 tank add 45 gallons of distilled water
and 50 gallons of water mother liquor from No. 54 tank. Start
agitator and heat to 80 C.

* 4* Add 595 lbs. of first grade crude crystals and

50 lbs. of residue crystals and dissolved, ‘ ' ~_>f ,

tW 1 ®!

r

WZ

5. Add fiC lbs of Darco and nix? we o :

6. In ease ‘there are no residue crystals the batch la com-
-pleted with first grade crystals. 1;.'* * v '^

V-.;.. Distilled water Is used when there is a storage of* water',
mother liquor. - ‘ *•’ .

:f $rr\ ‘~V+ Check filter press No 46 be sure that It Is In operating
condition. Steam should be on all trace lines and heating elements
In press. . *' * -V

8 • 8tart circulating pump No. 46 A. and circulate water •
solution through filter press No. 46 to top of No.41 tank.

Continue circulation untillall Darco has been removed
from the solution. . •. ; .V. ,

9. Fill jacket to cryastalliser No. 50 with water and
heat to 60 C.

10. Turn steam on tracer system from filter press No. 50.
cryetalliser, these lines remain heated unless flushed and drained .

1 1. When water solution is free of Darco pump to cryst-
-alliser No. 50.

12. Stop agitator on No.41 and No.46-A. pump.

Caution: Do not turn steam off of heating system
unless flushed snd drained*

15. Start slow speed stirrer in crystalizer No. 50 and

starts cooling waterto jacket. Cool oharge at the of 10 C per. hr.

4 - ■

cool to 20 C. Care must be taken to avoid sudden cooling since
rate of cooling governs crystals size. It may be necessary to -
vfaeed* the batch to start, crystallization. This ie done by
* introduclfcgn several crystals of pure adipic acid to the oryataliser
’ ; 14. when the solution in crystallizer No.50 has been

I

evolved to 20 C. and crystallised it is ready for centrifuging.

15. Place refined adipic acid crystals reciever under
centrifuge die oharge. ..

wmmmsm

16* Ci.*;rifuglng Is done on the blowing '*yclai

(A* Set liquor valves to water mother liquor storage '

So. 54. - _

■ ^ Start centrifuge on alow speed and chargefrom V

VW 60 ©ry stall! ser. when cake begins to build up near the^top^:
of the basket stop flow from So. 50 crystallixer. 4* /

fCjOPut centrifuge on high speed for one ■innri
<P0 Put oentrifuge on elow speed and wash cake with ^
three gallons of water-distilled. V',

(SO Put centrifuge on high speed for one minute* ‘if
(P) Put centrifuge on alowvrspeed and discharge VI. ’ '
crystals to refined adipic acid crystals receiver. .

The above cycle is followed untill crystalliser
Mo. 50 is empty. A full charge of approximately 500 gallons lii -L'- V .
So. 50 should be handeled in Sight loads in the centrifuge. . ; ~ ■ -

I/Z. ftrylng of adipic acid . " y. v j: ii-

The drier So. 56 provides for this operatlonnie a counter-
current rotary drier. Air heated to 140 C. by passing over steam
colls, is drained through the drier in one direction and adipic
acid Is fed in at the other end. '

Dry refined Adipic acid crystals are discharged at '
the other end. ...

The drier is of eufficient capacity to handle a twenty-

four hour make of refined wet crystals in six hours. The actual

performance of drier and rate of throughput must be adjusted , by ^

1 C. Recovery Bvapoatori .

— - ■ ■ - ■ - .'" 4 ;

The portion of water mother liquor in So.54 tank
which is not needed for dissolving crude adipio acid la pumpod ’-
to recovery evaporator Ho. 60. ,

The cwAte* and acetlo acid are evaporated "to the atmoephere
through the vent. The extent to which the evaporation 1* -carried
should be determined by ooollng a aample of hot liquor and notj
the crystallisation occurs at 20 to. 25 C. t the e vapora 1 1 on Is j -
stopped and the hot liquor discharged through • heated line
erystalliser Ho. 50. The crystallisation and centrifuging .of .^^ .
recovered adipic adld Is the same as in Part B. above '^*^7 ^ 7;!

Analytical Procedure: . - . " -If. ^ ~i*-Wy

•. The pure adipic acid can be analysed by dissolving,-^ 7.
a 1000 gram sample In methanol and tetrating with Q.5H caustic ‘/>
in methanol solution to the phenol -phthaleln end-point. -
% Adipic acid equals CC H base .075 100
-V wt. sample. '' :

A tjrtratlon of the base agalnstj^.5 HH£L should be run ~

for each determination.

A

Part *5 . ft^ocov ery of Acetic acid and Adipic acid from y r. t
the Purge Liquor. . 7 . 7777 -

Outline of Process: ' . 77 '•

Lactone acids are formed as by-products in the liquid .7^
phase oxidation, these are soluble In the solvent medlu’m and -
are purged from the system to prevent building up. The part of
•old mother-liquor which is not reoyoled is oharged to the wold
recovery still. Aoetio acid and ketone are recovered at the Wi".
.head nf the atlll. Lao tone acids are removed when adipic acld’JS'

Is centrifuged from therresldue liquor.

A flow diagram Is attaohed, figure 8.- |

Operating Proc(y-ure: O

A* Acid ^Recovery Still*

&

'fl!

1* Charge acid recovery still kettle No.53-A ifco ~"Y;. -
approximately one inch from the top of the sight glass with y-j;
acid mother liquor from So. 32 tank.

2. Turn water on oondenser No.33-C. v -

3. Turn steam on coils to So.53A. The full steam Yy.
flow may be applied -tatij^ the base of the column begins to warm
up. Then reduce steam flow to about 100 pounds per. hour and ..
establish reflux.

Turn steam on tracer to discharge line Mo.S3A

to hold-up tank So. 54 and heating coll in So. 34. Leave heat on

this system at all times unless completely drained. / ~ Y .

6. ■ The following cuts are made: ’■* . *

A. Ketone, water cut at 5:1 reflux ratio to

ketone water layer storage So. 6 (approx. 4 gals.)

6. B. Weak acid cut at 1011 reflux ratio. This

is drained from the receiver to a carboy to be discarded.-

(approx]5 gal) *’

C, Strong acid out at 1:1 rellux ratio ’to ■

receivers 33-E and 33-P and then dropped to pure aoetic acid y

etorage So. 13 (approx. 156 gals.)

, X). The residue is discharged to So.34 hold-up

tank.(a£prox. 34 gals) * ' “ T"--.

6. When the required strong acid has been removed

!# out off eteam and discharge hot residue to No. 34 tank* YYlyi

y'fs?"- 7 . Turn water off condenser No. 53 £• (Cautions Y

Leave small flow of water on this condenser In freezing weather

! ■ A

or drained completely). Since aoetic acid freezes at 16C. care

* * ♦ ai-TTciwy S59 "»o.t^ yo

must be taken to avoid plugging the condenser and draw-off lines.

y

, ‘K'r: : v *

Steam addil^jn to the ©ooling water ah?^).d he used when !
the raw water temperature ia b el oii^l6C? ^[!he draw-off and reflux
lines should be completely drained during shut-downs when the
atmospheric temperatures is below 16 C. The quality ofacetic
acid produced is eeheeked by the operator. \* . X -

A|20 cc. sample of the acid is titrated with 1.0R. H qjp B ■■'r.’; .

• • . r" - , - >y *

to the phenolphthale4n end-point. v- :

CalculatlOn: . ^ i - - - -

oo of l.ytt. Ka_pH 2.85 equalap acetic acid. s. ■■

B. Adipic Acid Recovery from the acid etill residue *Vr v ;

1. The acid still residue in Ro.54 tank la pumped
to crystallizer So. 50 and crystallized as instructed above for

acid mother liquor. ' 7 V* "

# - - -

2. The adlpio acid crystallized from the residue V

is centrifuged and washed. The mother liquor is discharged to ^
a drum for burning . '

S. The crystals are washed with 3to4 gallons og -
water. The water is discharged to the sewer.

4. Discharge crystals from centrifuge to residue I
crystals storagq. These crystals are reworked with first grmde
crude crystals to produce pure adipic acid. , " ^ .

V

w"

Wijis®

a? JAb/W-:*

UA//PS JW/7/0*

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correspondence, and are in the handwriting of GOLD, BOB PERSON, and >-

1E?UK. . ■ -- r .. r i : • ^ - a V-C ? * ? •

OOID stated that these papers acre another group of the amorous papers ha . r'j-^r.-'V
took hoae Just before he left the employ of BIQTHMAN. At about the tine .

BROTHMAJJ was having his showdown aith the other members of the firm, OOID v:-.

told EROTHMAN that he wanted about two aeeks to go orer all of this material
and asseable and annotate it. Subsequently, EROTHUAM told OOLD that the ■ : -'J - {?*&
laboratory was locked to OOID, so OOID Just kept the material.

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fHMAN & ASSOCIATES

6

A. BROTHMAN & ASSOCIATES

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subject^ . ' — ’ ' ' — ’ — : ■

ssssss

CABLE A0DKES9:
ftCSTCA KEUNtH.&AYVlUX.ILT. '
A B C. COO E crnnoM

SAYVILLE * NEW YORK

November H, 1947

. Tk

' 1 /

*»

A. Brothman and Associates <

2928 41st Avenue
L.I.C. 1, Mew York

Attention; Mr. Harry Gold. Chief Chemist
Dear Mr. Cold:

Thank you for your letter and inquiry of Hov. 10, 1947.

Under separate cover, we are sending you samples of our
different MICRO-CRYSTALLINE V.AXES which our chemists feel will ful-
fill your specifications. On these waxes, we quote you as follows:

HIGH MELTING POINT MICRO -CRYSTALLINE WAX 180/85 m.p.

PENETRATION 10-13 y

COLOR M.P. A. 3-4 '

# 15$ t per lb.

(for quantities not less than 500 lbs.

peSetratiS! G 8 H>i,,t 190/95 ’

COLOR 1 3-4 .-"*"1

6 25 * per lb.

(for quantities not less than 500 lbs}

HIGH MELTING POINT MICR0-CRYSTAI<LINE WAX 190/95 m.p. - -iV- -
PENETRATION 8 *

COLOR: WHITE . • - . ‘

§ 40* per lb.

(for quantities not less than 500 lbs}

k

t>Bter keunen MANUFACTURING CO.

c

- 2 -

:o

MICRO-CRYSTALLINE WAX 900 YELLOW
MELTING POINT X65/70
PENETRATION 35-40

-• 1M Pe r lb.

(for quantites not less than 500 11

Packing of the above mentioned WAXES is in Slabs or Cartons*
F.O.B. Sayville.

Delivery on all of these WAXES is Prompt.

If you have any further questions in regard to oar
waxes, please do not hesitate to contact us immediately.

Hoping to be of further service to you in the near
future, we remain.

Very truly yours.

cc:

SOCON Y-V ACUUM OIL CO M P ANY

INCORPORATED -t _-V^- ! >

230 Park Avenue, Sew York IT, N. Y. “ - _< : ~c't

1. Brothman & Associates
£928 - 41 Arenas
long Island City

i Attention : Mr. E. Cold

loveanber 24, 1947

Dear Mr. Goldt

^ Tour letter of Hovenber 10th addressed to our £6 Broadway headquarters has

"been referred to this office for reply.

Ve would prefer that you be nore specific as to the particular type of
Micro-Crystalline or Paraffine wax that you desire. To aid you in this selection
we have enclosed several technical publications regarding the application of waxes •
In the paper industry.

- r '- ' ' « r " ^

Me feel sure that these bulletins will be of interest to you and we look ; J
forward to bearing from you further. ' _ .; u -

i V As you probably know, the supply situation in regard to Micro-Crystalline^

and Paraffine waxes is extremely tight and should your interest be in any one of our
products, we cannot assure you that we would he able to make deliveries.!,.

If we can he of any further technical service, please do not hesitate to
©on tact this office. — -- ■ v

^ Tary truly yours, \;'.;uV:v^

V" SOCCan-VACUTJM OIL COMPAHI * -v"

Robert S* Shale

Process Products Engineer .

o

Jt. Broth man & Associates

2928 - la Avenue

Long Island City 1, New York

Gentlemen:

Thank you very much for your interest in our N-525 Neoprene Paint. In
compliance with your recent request we are forwarding to you, under
separate cover, a. laboratory sample of this material for your evaluation.

We are enclosing, herewith, a technical data sheet outlining the pro-
perties, of this newly developed compound which is presently priced at
$3*00 per gallon when purchased in drum quantities, $3*25 per gallon in ;
5's and $3*50 in single gallon containers. All shipments are made
F. 0. B. ( Cambridge, Massachusetts at our established terms of ten
days. . ..1

We would very much appreciate hearing from you after you have had the
opportunity of evaluating this sample. . .

Very truly yours

EHA:pn

end.

cc: H. I. Bar bey

k

V " : V C-525 NEOPRENE PAIHT O

DESCRIPTION: A solution of neoprene in an aromatic solvent with the addition
of other materials to yield a chemically resistant paint.

GENERAL USE: As a coating for the protection of surfaces which are subjected

to exposure to fats, oils, and greases or corrosive chemical -

liquids, solids, or fumes.

STANDARDS: Solids - 36 %

Specific Gravity - 0.?b9
Wgt/Oallon - 7-9#

Color (film) - Translucent, amber color

mSCIEEE SOLVENTS: Thinners - Aromatics, Ketones, Esters, Chlorinated
_ Hydrocarbons

Diluents - Aliphatic Hydrocarbons, Mineral Spirits,
Turpentine

SPECIAL FEATURES :

Shelf Storage - 2 months

Drying Speed - film loses tack in 20-30 minutes at room temperature
(65-75°F) and dries completely in several hours,
requiring no oxidation period.

Odor (film) - None

Chemical Resistance (film) - to acids and alkalies, oils, fats,
waxes and greases - excellent.

Durability - Excellent resistance to abrasive action; rubber-like
film will not chip or crack.

Adhesion - Excellent to wood, metal and other smooth surfaces.

APPLICATION: Bo special treatment of surface to be painted is necessary. How-

ever, the surface should be free from dirt, grease, rust, or other

foreign materials prior to coating. • ^ ^ -■ r

The paint may be flowed on from a full brush, avoiding as much as '
possible the re-croBSing of partially dried painted areas so that^
a smooth continuous film is obtained. A surface free from gaps,
ridges, and pinholes will prevent chemicals from penetrating be- .
neath the paint and causing localised attacks which may spread ■
and lift the film. If large areas are to be coated, adequate wen-.. -
tilation during drying should be provided. Drying at elevated
temperatures should be avoided to eliminate air holes in the film.

The paint may be thinned with toluol or other thinners if a spray .,.,,-
method of application is desii'ed. - ~ ;•

•

•

^ 21 fiup 47

i . ' - ,

A.

BROTHMAN & ASSOCIATE^ > i/tf

Chemical and Mechanical Engineers | / 1 (J 1 fit

114 EAST 32nd STREET 'ffli/.:'

’ NEW YORK 16, N. V. ^

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Cost UBCCX ABC Bth Kb. tmw
•tmin •■COMB PHBABB

•pmBTi Coanm

DISTRIBUTING AND TRADING COMPANY, INC.

444 MADISON AVENUE*

MEW YORK *2. M-Y. .

December 4 , 1947,

A. Brothnan Associates
86-03 57th Ave*

Elmhurst, L. I* .

Attention: Mr. HariyGold - "

Gentlemen:

With reference to our letter of November 14
and our sample shipment consisting of the following
material \

"DEETEE" American Ozocerite White 150/155

"DEETEE" American Ozokerite White 185/190 *

may we inquire whether these samples have reached you?

We would appreciate hearing from you as to whether these
products have your approval.

If any of our other waxes listed in our
booklet are of interest to you, please do not hesitate to
•request samples of such types* - '

Assuring>you of our best service, we are

WG/ mis

I-

l

T? IF

- A.y - --

y. '• - . > £ " HON BAY STAYS C OHRIM! »/eA

PROPERTIES OF 60£ TERTIARY BUTYL HYDROPBR OXIEE ’ •

Molecular Mel£it
Speciric Gravity • ES°C.
Bolling Point , - %

Freeilng Point
Plash Point : "
Refractive Index M E5°E.
pH In 10^ eater solution
. Og available - i : ■-*
Color / '

Stability; ■' .'v V

m* Bp to 76.6° C ■
b. Above 76*6° C

M

indefinite • -

decomposes at a rate proportioned
to the temperature* .

Activators; . ~ -r- ~ - i; "- ^

Hydroqulnone and other like organic reducing agents have proved bo
be efficient activators when used In quantities up to 0*1 of TBOg*

Solubility;

In Mater
Mater In

Short chain allphntlca
Aromatics

11 %

€%

Excellent

Sxcollent

Price Bet-up:

$3*00 per lb* up to £79 lbs. .

1.50 per lb. £79 lbs. or nore w'

BUREAU OP EXPLOSIVES REPORT FROM CHEMICAL LABORATORY '

The material Is a water white liquid with a Specific Gravity Of
O.B60 at 15°. C. It has a sharp penetrating odor that would serve tsa . .y i; r
a warning In caso or leaking packages*

Tho liquid is stable through prolonged heating at T5° C and did not ‘ * .
decompose violently when hoated up to 30C©c* Ho notlcoable pressure
dovolopcd in a tightly closod bottle cStar .standing five days ot laboratory
temperature* . \y- * .

The material Is readily lmTlainmblo when lgnltod, Tho combustion ©T
fine organic material saturated with the liquid Is accoloratec somoihat - V
but not dangorously so* Tho notorial falls to explode when detonated ;

by a blasting cup* ...\ v _ ; . . . \

. The flash point was determined as 62° P. This notorial Is classed as

tn Inflancxiblo Liquid and is consldorod sufficiently safe for transportation*

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/ yL «_ ^-^U. rrw T* _£f^L o. TJU*

XR-31C0 and XR-1 i357 , - \ V

■/ - The unmodified resino, XR-31C0 and XR-h357, are tough, pale colored. -

and have exceptional resistance to rr is tore , alkalis, acids, oils and greases . ,

They impart high gloss, easy polis'iing characteristics, durability and fhoodont
from water spotting to nitro-cellulose and ethyl cellulose lacquerc. The ■
flexibility and real stance properties of the XR-Ja 357 have made It excellent - yr, . „
for use in adhesives and plasticisers. - * .

XH-310O ( « . . -• . • V.

X permanently fusible resin having high alkali, acid, water and grease
resistance. It gives high gloss, remarkable depth of luster and fiillnoss, fair
color, and extreme resistance to perspiration. It has a very low acid value.

It requires combination with nitro-cellulose or/and ethyl cellulose for solution ^
stability. It will not cook with oil. , . .. . L . ...

It is used in both interior and exterior lacquers, lacquer coatings Xbr .
paper and cloth, hardware lacquers for perspiration resistance, and auto-re finish-
ing e namels and clears. Color retention is fair. . ...

Typical us ob are fer product finishing lacquers and for exterior lacquers,
clear and pigmented. Advantages: — high gloss, gloss retention on exposure (less
chalking), good adhesion and non- tarnishing in clears over metal, resistance to
moisture and water e petting in auto enamels, high durability, resistance to oils
and better fat in refrigerator lacquer tests, non-yellOT.ing. An iuq»rtant
property is its ease of polishing to a hfgh gloss. , < ~

,T. v --Clear lacquers, based on the folio wing proportions, have given good

durability In exposures.

ITOOCrUriDnE H3SIR

FUS7ICIZ31 (dibutyl
phthalate)

0.5
0.3 -
0.1

The XR-31D0 is in itself fairly flexible and requires less plasticiror as larger
proportions of rosin to cotton are used. The lacquers become slower drj'ing and
softer as the proportion of resin i3 increased, 1 1/- part® of resin to 1 of . .
nitrocellulose approaches the Unit for general hardness. /

Properties*

Color:

Resin
. Film

Specific Gravity
Jfclting Point
(Ball t Ring)

% ffen- volatile
Acid Humber

2-^I(3tl xy'lol) '
Very e^od to fair.
1.30

125-150°F. •
1002 .

1-3

c

o

61

- 2 -

iH-U3g7

Xfi-1357 ic slightly softer and darker in color than IR-3180. It has
excellent adhesive qualities and is good for plasticizing other eolations. In
addition. It is used as an ingredient in adhesives and as a plasticizer far
certain of tbs dispersion resin costings.

fropcrtiaa t

Acid So.

Color

Oil solubility
Belting Point
Specific Gravity
T/eigbt per Gallon

Stability of Solution

T7e do not offer a solution of XR- 31 C 0 for sale*

Cold cut solutions are loss stable than thoso oade by beating. Cold
cut solution in cotton solutions or solvents that arc cloudy when cade, are
certain to be unsatisfactory. In any precipitated solutions, the original con-
dition of the solution race by boating $0 restored unchanged by warning up the
separated dx and stirring at li*0° F. to bring about re-solution.

.Settling of an XH-JlDC solution should be viewed as crystallization and
ray be prevented by the use of nore powerful resin solvents, by proper dilution
In these solvents or into a finished lacquer pronptly after making up the solution,
or by the use of temperatures high enough to prevent itB starting. ?7ith slight
alterations in final properties, 13-1*357 designed for stability of eolution, nay
be used.

Hot over 1.5
>9

Poor

Approximately 117-121°F.
i.2b

10.3 Ibe.

Regarding the order in which solvents rank as to power end keeping of
solutions, there is no numerical rating possible. However, the following list
of solvents and other lacquer materials are given in the order of decreasing •

solvent power of toleration.

Solvents

Uon-Volatile

Acetone

Tricresyl Phosphate

rthyl Acetate

Dibutyl Fhthalate

Toluol

nitrocellulose

butyl Acetate

Phenolic Resins (Bak elite)

Xylol

Natural L Modified Resins

Cellosolve

Oils

Alcohol

Petroleun Tliinners

The most unexpected el tuition in this listing is perhaps that alcohol* ~
are such poor solvents for XR-31C0, Petroleum thinner® very markedly, some, such
as the Solvessos, haring about as good toleration as the alcohols* The usual - -

mineral Spirits, however, are oompletely ismiiacible.

Lacquer* or resin solutions in which the combination contains the tolerable
limit of oils, alcohols, petroleums, etc., are the most troubleoorie for precipita-
tion. 3e have had no instances in which lacquers, made up to 25 - 35 % solids with
acetate and benzine series cf thinners, have separated on two to throe years
Storage, avan when the solids were largely XR-3I8O. Equal parts of 3180 and
toluol will precipitate in 10 to 30 days. A solution of two parts of toluol to
one part of resin will norcally last from several weeks to several months, and
one of aqual parte of toluol, ethyl acetate and resin will last somewhat lci^or.

Mote t 50> solutions of XR.-3180 in the stronger solvents must contain a
little nitrocellulose, ethyl cellulose, alkyd, vinyl or other resin to stay in
•olution for definite periods of time. Solutions that are capped and not continu-
ally being disturbed seem to be most stable.

Discoloration of XR-3IOO in Lacquer

While X.1-3100 re Bin alone lias little or no tendency to discolor on ex-
posure to light, when used with nitrocellulose, the combination yellows more than
either one alone. This discoloration depends on the intensity of the light; is
greatest under the U.V.Aro, less on direct exposure to sunlight and still less in
diffused light.

Very satisfactory white lacquers have been produced ibr indoor us© as'
regards color or discoloration.

Any ^udgnesnt of color change should be made on the basis of equal gloss
or gloss retention, XS-31CG will perndt higher pigmentation far equal gloss as ..
compared with Danmr. Tho glcss retention of XR-31SO is also excellent. TThila
XR-li357 holds gloss still better than 31C0, the XR-3180 will collect less dirt
on outdoor exposure.

Plastic Checking

XR-3180 has a low melting point and when used excessively in a lacquer,
mill lead to plastic checking on exposure. This tendency say be reduced by using
a moderate aaount of JK-31C0 { 50 - 65 % cf solids on the average), and plasticising
to suit the conditions. Any modification with hardening or stiffening agents, ~
such as hard or rubbery resins, pigments, especially of the fibrous type, cor
higher proportions of cellulose ester, should be effective in reducing plastic
checking.

J*ob a durability angle, XR-3180 does not see® to bolster up ester pun. -
Snell percentages of XR-31B0 give very little or no increase in life of the filau
This nsy be due to poor compatibility and would apply eq ually to Daaar,

The oocnon lacquer rosins are barely tolerated by 501*3180. The alkyde,
lUcar, ester gun or rosin containing resins generally give hazy solutions at best
with XH-JLSO. IH-3180 is probably the nest conpatible with cellulose of the
above resins, and in sone ways, almost resembles a solvent in its action*

Resins that readily combine with XR-3100 are less compatible with nitro-
cellulose (viqyls, styrols, etc.). Excellent compatibility ®ay not be necessary
for mixing to give the desired results.

Also, plasticizers wlilch are not compatible with XR-31C0 cay not rule
out their uso (castor oil being an exception). Tricresyl phosphate is & solvent
ibr 31XJ0 and dibutyl pbtbalate nates an excollent plasticizer.

The following formula suggestions cay bo of interest to you:

LP-8205

LF-9D59

LF-9170

XE-7172

B3-3Q2 »

This is viscous oil-modified resin which has a fairly deep yellow 00 lor
and a phenolic odor. It gives low viscosity in laccuers and may, therefore, be
used with larger proportions of higher viscosity nitrocellulose than usual. -
Gives clear and pignented lacquers of unusual durability, body and water resistance.
Dae to color used only where yellowish Clear is acceptable or in dart and solid
colors. Despite color and odor its high integrity in lacquers still continues
its usefulness In specialties.

Properties

Color —

Specific Gravity —

Viscosity —

Solids —

Keeping Time —

Compatible with —

lib-6 (3*1 xylol)

1.02

200-360 cp (3:1 xylol)

100 %

1 year

Nitrocellulose and bitumens

BJ-16580*

This is a non-oxidizing, heat-reactive C-9 {"Garble" anhydride) type
resin wlrich will cold blend with nitrocellulose, ethyl cellulose, chlorinated

rubber and urea resin; to give non-yelloring films haring a high order of ' ~

flexibility, adhesion and solvent resistance, BJ-165DO acts as a resin plastic iser >
ft? both lacquer and urea yielding a tough filn with excellent adhesion along with ■ -
alcohol resistance and durability. Excellent fbr paper and cloth coatings of ill-' - '

typ : ;vj> ,

t

Acid Bo,

Baking tine (alone)
Color

Solid content
Specific Gravity
Viscosit}'

Keeping Tine
Solvents
Thinners
Wt. per Gallon

— 21 - 3 1 * " :'rr~Z-2'::Z

— -30 Kina. U 250^F. i '

— Sot darker than Z ^

— 0o< • V v'*' :Tj ?**'■

- ' l.os (as is) - 3

— 200-hS0 cp. (3 si xylol) Ti; /

— 6 months or longer -v bv.-;

— ^loi ' - v ;•••

— xylol-Solvesso, ethyl acetate

— 6,3 lba, .

F

,TBE PREPARATION OF URSA FORMAWEBTDE COIX^A

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> following is 'the procedurw for the preparation of the vr&-J%3§$ *
cold-setting glue: : ,,; ' v. -. <Vr ^y .-; - i ~ y .ily p - ,;

•Tliter#’ three-neckcd flask immersed to batcb-content-level juB^*^^

aiuter, xnree-necicea r±asx immersed xo oatcx»-conw«n^iBvoi .

iyi-iy r ~. % l»ttf JpppaSjLe of maintaining the batch at a tempera tore between 20° „

jfe-ft Jr.;’ T 25 °i;.V l *dd 1 J 622 gms. hf 37% by weight formaldehyde-in-water .aolatiotuv^^:^ 5 ^;'^
v 1060 gms. of.irea should be added to the formaldehyde, under -agitation* \ \

The solution' hould then be corrected to a pH of between 7*3 and ' 7*5 *T ; %^1'J^zLt ' ■* 4
p^rfV ,: : ; “ the addition t approximately 13 ails. IS NaOH, the amount depending'upon
Ljf ^ i the initial pEof the formaldehyde solution. The reaction Mixture should J

*be Maintained X thin the specified pH and temperature levels for a .period, Vy,;!

-of 21 ; hours. 4t the end of this time the conversion of formaldehyde and T ; y- J ^lV i
' '[ urea to aethylb. urea and dimethylol urea should be virtually . quantitative*,: 2 %^ >i

§•'', .,‘ 2 -. ^;:V' .'• ‘ ‘ y : v - >* - . • ■•• „ o-riyy. \.vvL.‘."

- The Bolutin should then be adjusted to, a pH of 5*0 hfXbe '

WH-' of approximately ?6 cc. of IS concentration acetic acid. The temperature -
of the Mass shofci be raised to reflux temperature in a period of not More
than 30 Minutes J The solution should then be adjusted to a pH of *q>proxi i
aately 7 to 7*5 V the addition of approximately 1*0 cc. of IN NaOH. 1

solution should lien be concentrated to 70j re sins-in- solution concentra^'^aiv;^^ 4
*pi-f -t* J - tion under a vacia of 200 to I 4 DO ram. of Hg. At this point the formation
of the resin gluetmlution has been accomplished. .rf~ •„ —

_ The preparation of the glue mixture involves the following procedure* -yiy .■ j

\ /. \ v - . . - ;

f ' 1 - To 100 gms. ol resin glue solution add 2 gats, of walnut shell flourv :y ?\ V
The walnut ah ell flour should be added progi^ssively and dispersed as well : !ey'; ' ^
, as possible in the j^lue solution. This can be accomplished by hand-stirftng, j

employing a glass ri in a beaker, when walnut shell flour of +200 mesh to %

-300 Mesh is enp>loy«. The proper dispersion of the walnut shell flour - ^ ; ' - J

depends on the addi-tan of the flour at a rate under continuous agl tation
such that at no time is there a significant amount of walnut shell flour "SWk^Jll^vT^
-present in an undi^srsed fora. r

'■ To the thus peered flour-and-glue-solution dispersion, there •;'* & k
should be added 1 cc [ of * water solution of 11. 5 gms. of ammonium chloride*’''- y ”, , -
1': j .in 250 cc. of water. This catalyst Mixture should be well dispersed in ~ ~

r^7^^*? U& " solution di8 P ersion ^ the resulting mixture should than be 3

; ^ rest for one and one-half hours. This mixture should demoiistra te, -- V: /'

»». - ... “ e ond of the mentioned one-&nd one-half hours, a pH of about &.S

-• .. 5.-..:--.. w-rv: ;- s ^

.. . *“ e £^- ue »ixture should then be dpread between the yellow ’v»£& i S& 3 »

Kfi h c? e f e ^r' pane:Ls ^ ompris1 ^ the ultimate plywood composite board, *

jhat ^hto 2$ gms. of glue Mixture ase spread for each square foot of 4

' ?^'lI h ®, P S r V ehoad y 100 h® P Uc «* in « press at 100 psi pressure for^f^S^ *
: ' -° f hours 60(1 “aintained at a temperature of 83 F* for «b . i

t.I , f.t tie end of the 2 J| hours the resulting plywood should T . -

to cure at a temperature of not less than 75 F* for a period' of sir ■ "'> • ”

Wa. At the end of the specified interval, specimens ®ay be cut and pre- > vv V- .

... . .pared for testing. . r/ r .. - - ^ * ' ■’* ^ '■ ■- y

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On Jum 2li # 1^50 GOLD Advised that the haixbrriting <m the t»o sheets
of paper In this folder vu hie tnmtnd that it was concerned 'With
library work on January X># l?lj w hi c h he did in connection with
Titanic work far the Pennsylvania Sujar Coopaqr« -3 a V-':r v ^T- V >«*V:

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On June 24, 1?50 GOLD advisod that the material in thin foldcsr wa.
* n Mn hanctariting and consisted of laboratory notes on Mr ‘■ask
on 00 2 recovery at the Pennsylvania Sqgar Cotapaiy. ^ .<*

On the sane date GOLD identified the above folder a* containing ^ -
assays in connection with his work at Pennsylvania
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T. SCOTT KILLER, EJL

BAHHT GOLD
ESP- E

654J 07-13 1 2 (li) Folder Up. 12

Ob Jane Pi;, 1^50 GOLD adrised that mtaae of the material In this
folder Is concerned with Titarsine in connection with GOLD’S work
mi Pennsylvania Sugar Canp&i^. The report dated 12/5/1+0 was
material on production of lactic acid and a page entitled ■parronal
Affaire* with the follow!^ written thereafter in GOLD** handwriting*

V another job
b. more dough here
o. own laboratory
d, debts

Attention la called to C* above which indicated that GOLD w e «
considering a laboratory of hie own as well as D. above which
indicated that OOLD had debts. GOLD has advised that he was continually
in debt because of hie expenses in Soviet espionage.

GOLD said that the letter dated V22/1+2 vas in the handwriting of
mnRBm.T. £, IDUGHEHTI and was a work prograa far Hr. EOCH.

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On Juno 2li, 1?50 GOLD Identified this rffiterial as work be did "V^'K^v"- v
at Pennsylvania Sugar la connection -with a book '■bleb GOLD was s

going to draw up for Dr* HUTCH end which was concerned with *,

JtenqylraniA Sugar Ccnpaxy Methods* . • • . *~:;v.r •*>-*.- vrV^'v^^.r* ~

OOLD alro eta ted that thle folder contslned yltaain tssay mtoriA'X^Tr&X, }
In connection with GOLD*c -work at Pennsylvania Sugar* '■ . ' ’

On the Mae date 001D advieod that all of the material in this ? V:-
folder was concerned with Titanic aeaay work he did at FannEylvania
Sugar* . . ‘

TS’dtEUC